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Thin SAPO-34 membranes synthesized in stainless steel autoclaves for N2/CH4 separation
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Development of Additively Manufactured Complex Tools for Autoclave Cure Composites
IACMI Project 4.9, Tooling for Composites with Washout Features Produced by Additive Manufacturing, assembled a team including the industry lead, Ability Composites, NREL and Colorado State University (CSU). Ability Composites had originally expressed interest in alternate methods of producing tooling for composite parts. In follow-up discussions, it became clear that one of the bigger tooling challenges revolved around small production volume composite parts that were tooled on washout material due to the complex geometry. To build an understanding of the potential, both from a technology and a cost perspective, for replacing conventional washout tooling with 3D printed thermoplastic tooling, a number of commercially available dissolvable FDM printing materials were evaluated, leading to tooling representative of commercial articles of interest to Ability Composites. Ultimately, Ability Composites was able to directly compare autoclave processed prepreg composite parts produced on conventional washout tooling to composite parts molded on 3D printed dissolvable tooling produced at CSU. Small, laboratory test specimens were developed to investigate the structural performance of the candidate materials under autoclave processing conditions, which were nominally 121 °C (250 °F) and 345 kPa (50 psi). In addition, several internal structural configurations (infills) were evaluated under autoclave conditions using model materials. The results of these tests indicated that two materials, Stratasys ST 130 and Infinite Materials Solutions Aquasys 180 (AQ 180), were the best candidates, given the specified autoclave processing conditions. ST-130 was slightly more robust than AQ-180; however, the AQ-180 was carried forward as it was dissolvable in water, not requiring the basic solution needed to dissolve ST-130. Based on the preliminary material and 3D printed structures evaluations, larger tools with a truncated square pyramid geometry were created to produce prepreg composite test articles for 3D printed dissolvable tool evaluation under standard autoclave fabrication conditions. Two tools were manufactured using ST-130 and one tool using traditional ceramic washout tooling media. The tools were evaluated for geometric fidelity and surface roughness changes before and after carbon fiber/epoxy prepreg composites were manufactured on the tooling. The autoclave processing did not impact the geometry significantly and was completed at 121 °C and 345 kPa, indicating satisfactory tool performance. The results from surface roughness testing of both the resulting composite and the associated tooling indicated that an adequate surface resulted without the need for a surface sealing step, as was required for the conventional washout tooling. Based on results of the truncated pyramid tests as a basis, ST-130, AQ-120 and AQ-180 materials were carried forward to the tool geometry of interest to Ability Composites. These hollow rectangular bent ducts, which were complex in nature and not extractable after cure, were used to understand the impacts of tool material and thickness. One ST-130 tool was produced as a partially solid part, with an enclosed 40% dense infill region to reduce weight and material use. This was the same approach evaluated in the truncated pyramid portion of the study. This tool was to be envelope vacuum bagged and directly compared to a monolithic tool of conventional washout material. The traditional monolithic ceramic tool was manufactured by Ability composites using CNC-based subtractive methods. An additional five dissolvable polymer tools, manufactured from ST-130, AQ-120, and AQ-180, using a hollow design were 3D printed and used to produce carbon fiber/epoxy composite evaluation articles. These hollow dissolvable tools were expected to be less influenced by the autoclave conditions as the wall was solid and vacuum bagging was inside and outside the tool. This alternative geometry was also evaluated as an option in techno-economic modeling. Print times were reduced from in excess of 3 days to under 30 hours, while surface quality and and tool integrity were substantially improved in the transition from the partially solid tool to the hollow tooling concept. Ability Composites produced autoclave-cured prepreg ducts on each of these tools. The autoclave conditions utilized were more severe than those of the initial trials, reaching temperatures of 160 °C and a pressure of 414 kPa. Under these conditions, the partially solid 3D printed tool with skin and 40% dense infill crushed significantly; however, the thicker ST-130 hollow tool showed good promise, deforming only slightly. The thinner hollow tool walls were unsuccessful as were the other materials. Overall, the hollow tool manufacturing process saved significant amounts of time and material in manufacturing as compared to the solid ducts and produced composite surface quality improvements compared to the traditional washout tooling. The TEM was developed to allow direct comparisons between conventional washout tool manufacturing processes and those developed at CSU. It also allowed for two separate 3D printed tool geometries to be analyzed and compared. In this case, the square bent duct tool geometry was determined to be representative of common washout tools. This geometry was compared with a scaled-up version of it to assess differences in the two manufacturing processes based on tool size. The model was developed to make use of user input in the form of geometry details, process steps, manufacturing parameters, bulk material costs, capital equipment costs, and general costs to calculate overall labor, material, capital equipment, and energy costs per manufactured tool for the conventional and additive manufacturing processes for the two representative geometries. It was also able to estimate step-by-step process times for the manufacturing process and geometries. Based on significant input from Ability Composites and CSU from their knowledge gained from hands-on manufacturing of the 3D printed bent duct tool geometry, costs and process times were calculated for the two manufacturing processes. Results showed that the additive manufacturing techniques developed at CSU can substantially reduce the costs of tool manufacturing by reducing labor times and material usage. This is because additive manufacturing is a relatively hands-off process and allows for the tool design to be optimized to reduce material usage. The disadvantage, however, is that process times for additive manufacturing are significantly longer. The three-dimensional (3D) printing process is slow if tight tolerances are required, but the analysis did show that print times could be reduced with the hollow tool geometry. Also, further advances in additive manufacturing could expedite the process. Costs and process times for the tool washout process were calculated separately. They showed that costs are relatively insignificant when compared to the overall tool manufacturing processes, but with increases in tool size, costs for the conventional manufacturing approach are larger than for additive manufacturing. Again, the washout process for conventional tools is very hands-on, whereas for additively manufactured tools the print medium is dissolved in an automated detergent bath at the sacrifice of process time. The analysis showed that optimizing the additively manufactured tools may also reduce washout times. Overall, Project 4.9 demonstrated that commercially available dissolvable 3D printing materials exist that can be used to produce dissolvable tooling capable of surviving prepreg composites fabrication under autoclave conditions of 121 °C (250 °F) and 345 kPa (50 psi). An alternative hollow dissolvable tool design was developed which was structurally superior to the initial concept and was cost and time effective versus conventional washout tooling. The 3D printed sacrificial tool required no added surface sealing steps prior to composite part layup and cure, offering a significant advantage over the porous conventional washout tooling.
Autoclave treatment of the classical scrapie agent US No. 13-7 and experimental inoculation to susceptible VRQ/ARQ sheep via the oral route results in decreased transmission efficiency
Scrapie, a prion disease of sheep, is highly resistant to conventional deactivation. Numerous methods to deactivate scrapie have been tested in laboratory animal models, and adequate autoclave treatment can reduce or remove the infectivity of some classical scrapie strains depending on the heating parameters used. In this study, we autoclaved brain homogenate from a sheep with US scrapie strain 13–7 for 30 minutes at 121°C. Genetically susceptible VRQ/ARQ sheep were orally inoculated with 3 grams of the autoclaved brain homogenate. For comparison, a second group of sheep was inoculated with a non-autoclaved brain homogenate. Rectal biopsies were used to assess antemortem scrapie disease progression throughout the study. Five out of ten (5/10) sheep that received autoclaved inoculum ultimately developed scrapie after an experimental endpoint of 72 months. These sheep had a mean incubation period of 26.99 months. Two out of five (2/5) positive sheep had detectable PrP Sc in antemortem rectal biopsies, and two (2/5) other sheep had PrP Sc in postmortem rectal tissue. A single sheep (1/5) was positive for scrapie in the CNS, small intestine, and retropharyngeal lymph node but had negative rectal tissue. All of the sheep (10/10) that received non-autoclaved inoculum developed scrapie with a mean incubation period of 20.2 months and had positive rectal biopsies at the earliest timepoint (14.7 months post-inoculation). These results demonstrate that sheep are orally susceptible to US derived classical scrapie strain 13–7 after autoclave treatment at 121°C for 30 minutes. Differences in incubation periods and time interval to first positive rectal biopsies indicate a partial reduction in infectivity titers for the autoclaved inoculum group.
An Artificial-Intelligence and Machine-Learning-Based Methodology to Conduct Seemingly Strain-Controlled Fatigue Test in a Pressurized-Water-Reactor-Test-Loop-Autoclave, While Not Controlling the Strain
In general, low cycle fatigue analysis of pressurized water reactor (PWR) components, requires strain-controlled fatigue test data such as using strain versus life (ε–N) curves. Conducting strain-controlled fatigue tests under in-air conditions is not an issue. However, controlling strain in a PWR-test-loop-autoclave is a challenge, since an extensometer cannot be placed in a narrow autoclave (typically used in a high-temperature-pressure PWR-test-loop). This is due to lack of space inside an autoclave that houses the test specimen. In addition, installing a contact-type extensometer in the path of a high-pressure flow can be a challenge. These difficulties of using an extensometer inside an autoclave led us to use an outside-autoclave displacement sensor which measures the displacement of pull-rod-specimen assembly. However, in our study (based on in-air fatigue test data), we found that a pull-rod-controlled based fatigue test can lead to substantial cyclic hardening/softening resulting in substantially different cyclic strain amplitudes and their rates compared to the desired cyclic strain amplitudes and its rates. In this paper, we propose an Artificial-Intelligence and Machine-Learning based technique such as using k-means clustering technique to improve the pull-rod-control based fatigue test method, such that the gage-area strain amplitude and rates can reasonably be achieved. In support of this, we present the fatigue test results for both 316 SS base and 81/182 dissimilar-metal-weld specimens.
THERMAL ANALYSIS AND DESIGN OF SELF-HEATING MOLDS USING LARGE-SCALE ADDITIVE MANUFACTURING FOR OUT-OF-AUTOCLAVE APPLICATIONS
Autoclave processing is a commonly used state-of-the-art fiber-reinforced composite manufacturing technology, albeit high capital cost, long cycle times and high energy consumption. Alternatively, out-of-autoclave processing reduces the initial and operating costs while producing composite structures with similar quality as that of autoclave parts. Additive Manufacturing (AM) the scaled-up molds for out-of-autoclave process using carbon fiber (CF) reinforced composite offers design flexibility, enhanced mechanical, and thermal properties in addition to reduction in weight and cost. However, heating of these molds using an oven is still expensive and necessitates an energy-efficient heating process. In this study, resistive heating through heating elements embedded within fiber reinforced composite molds is used as an efficient heating mechanism. The goal is to design wire embeddings and determine the optimal heat flux density to achieve a target uniform temperature of 1000C across the mold surface. To this end, numerical analyses were performed to evaluate the temperature distribution across the composite mold surface for a given wire placement and mold configuration. Constant thermal properties of the 20 wt.% short CF reinforced acrylonitrile butadiene styrene (ABS) were used in the thermal analysis. Time taken to reach the steady state temperature was also estimated. Design guidelines for wire embeddings were included to enable efficient manufacturing of fiber-reinforced composites through out-of-autoclave molds.
Optimization of the autoclave preparation process for improving resistant starch content in rice grains
Abstract The autoclave preparation process to increase the content of resistant starch (RS) in rice grains was optimized, and the results showed that the optimal preparation process was obtained with a water content of 41.63%, a pH of 5.95, an autoclave time of 60.96 min, and a refrigeration time of 17.11 hr. Under these conditions, the theoretical value of RS content in rice grains reached 17.57%. After autoclaving, the estimated glycemic index (EGI) in rice grains was reduced from 78.35 to 66.08 measured after cooking, suggesting that autoclaving was capable of increasing the RS content in rice grains and reducing its EGI value. These results may help spark new concepts and methods for the development of specialized foods for specific populations, such as people with diabetes.
Re-establishment of Sandia National Labs super-critical carbon dioxide testing autoclave capability for exposure of metal alloys and polymers (Level 4 Milestone Report)
The sCO 2 system located in 916/160A, Sandia National Laboratories, CA, was constructed in 2014, for testing of materials in the presence of supercritical carbon dioxide (sCO 2 ) at high pressures (up to 3500 psi) and temperatures (up to 650°C). The basic design of the system consists of a thermally insulated IN625 autoclave, a high-pressure supercritical CO 2 compressor, autoclave heaters, temperature controllers, gas manifold, and temperature and pressure diagnostics. This system was modified in 2016 (sCO 2 compressor was removed) to enable corrosion studies with metal alloys in gaseous CO 2 at lower pressure (up to 300 psi) at 500°C. The capability was not used much afterwards until 2020, when preliminary tests using this capability (again without the supercritical CO 2 compressor) involved the exposure of fatigue and tensile specimens of HN 230 and 800H alloys to CO 2 gas for 168 hours in gaseous CO 2 . Using this capability, we finished experiments with low pressure (450 psi/ 3 MPa), high temperature (650°C) exposure of fatigue and tensile specimens of HN 230 and 800H alloys to CO 2 gas for 168 hours. The data from these experiments will be compared to that gathered from experiments performed in 2020 using the tube furnace and presented in a future report. It is to be noted that the tube furnace experiments ran 500-1500 hours, unlike the 168 hours of exposure in the recent experiment. This can help validate the use of the sCO 2 autoclave for both CO 2 and sCO 2 experiments.
Investigating grid-to-rod fretting wear of nuclear fuel claddings using a unique autoclave fretting rig
Fuel rods in a pressurized water nuclear reactor (PWR) experience coolant flow-induced relative motion against the grid support features, a phenomenon called grid-to-rod fretting (GTRF), which may cause progressive fretting wear damage. Wear-through of the cladding on fuel rods will leak the radioactive fuel into the coolant loop to significantly increase the radiation level in PWR primary loop and often trigger expensive Post Irradiation Examination. In this work, a unique autoclave fretting test rig was designed and fabricated to allow studying GTRF using actual cladding and grid materials. Water temperature was up to 220 °C, which was designed to mimic the environment in an industry full-assembly reactor core simulator. The contact load (0.1–1 N), oscillation frequency (20–30 Hz) and stroke (50–150 µm), and work rate (1–3 mW) were defined based on simulations of GTRF in an actual reactor. Using this autoclave GTRF rig, tests were conducted to learn the effect of water temperature and to investigate the wear behavior of different cladding-grid material combinations currently used in actual PWRs, including Zr alloy claddings without and with pre-oxidation against Zr alloy and Inconel grids. Higher water temperature evidently increased the cladding wear, and pre-oxidation of the Zr alloy and/or using the Inconel grid effectively reduced the wear rate. In conclusion, results were correlated with the data of a full-size industry reactor core simulator in terms of both wear rate and wear scar morphology.
Simulation Assisted Design for an Additively Manufactured Autoclave Tool Accounting for an Anisotropic Expansion
Carbon fiber reinforced polymer composites have been used in Big Area Additive Manufacturing (BAAM) to decrease the distortion during the printing process and increase functional stiffness. These materials are also important for additively manufactured autoclave tooling which expands when exposed to the high temperatures of the operational cycle, causing the dimensions of the mold to differ from the targeted design. Since the reinforcing fibers generally align during the extrusion process, the thermal expansion of the composite along the deposition direction is restrained by fibers, whereas the thermal expansion perpendicular to the bead is largely unconstrained. This leads to an anisotropic expansion of the material that is dependent upon the local deposition path, which may be tortuous and complex. To obtain an accurate final part geometry during the autoclave process, a computational prediction of the thermal expansion of a tool is required to account for the complex extrusion deposition directions. A multi-step approach is presented that accounts for (1) anisotropic thermal expansion of the extruded bead, (2) the complex deposition directions, and (3) internal geometry determined by slicing software. The thermal expansion coefficient in the deposition direction and perpendicular to the deposition direction were measured at multiple locations in the test specimen. A revised model geometry was generated to achieve the target dimensions when accounting for thermal expansion.
Autoclave grid-to-rod fretting wear evaluation of a candidate cladding coating for accident-tolerant fuel
In pressurized water reactors (PWRs), water flow induced vibrations cause contact and rubbing between the fuel rods and the supporting grid, a phenomenon known as Grid-to-Rod-Fretting (GTRF). GTRF may produce progressive wear damage on the fuel claddings leading to subsequent leakage of radioactive fission products. Various accident-tolerant fuel (ATF) concepts are being developed for higher resistance to the high temperature steam and one approach is to apply a cladding coating. Here, fretting wear behavior of a candidate Cr-coating was investigated using a unique bench-scale autoclave testing rig mimicking the environment in an industrial full-assembly PWR simulator. The contact was under a realistically low load (~0.5 N) lubricated by deionized water at a temperature of 204 °C under a pressure of 20-23 bars. Results demonstrated that the Cr-coating significantly improved the cladding's wear resistance when tested against a commercial ZIRLO grid with or without pre-oxidization. In addition, the Cr-coating also reduced wear on the non-oxidized ZIRLO grid but slightly increased the wear on the pre-oxidized grid.
Autoclave Molding of Thermoprotective Coatings on Large Products Using a Metal composite Mandrel
Abstract—A technology is developed for the application of a thermoprotective coating by autoclave molding with a metal composite mandrel. This technology decreases the financial and labor expenditures in production. The proposed method is compared with the application of a thermoprotective coating by hydroclave molding.
Autoclave Corrosion Experiment of Zircaloy-4 at Temperatures Between 180 deg. C and 270 deg. C - 19167
Corrosion of zirconium alloys is a key issue for the overall nuclear industry that has been studied under various temperatures for plant operation, severe accidents, storage, and final disposal of spent cladding. The present work aims to investigate the corrosion kinetics of zirconium alloys at intermediate temperature regions between the operation and storage/disposal conditions, to examine if the extrapolation of high temperature data to lower temperatures is valid. To achieve this, an autoclave experiment, which is a common way to study corrosion behavior, was applied for up to 485 days at 4 different temperatures: 180 deg. C, 210 deg. C, 240 deg. C and 270 deg. C. The weight gain changes due to the oxide growth of the PWR cladding tube (Zircaloy-4) showed that the corrosion kinetics in temperatures above 210 deg. C follow the cubic rate law. The activation energy evaluated by the Arrhenius relationship of the cubic rate constants was determined and found to be 132.8 ± 0.6 kJ/mol, which corresponds to that generally reported under the operation temperatures. However, the kinetics at 180 deg. C was found to be close to the parabolic rate law, which suggests the kinetics changes from cubic to parabolic around 200 deg. C. Thus, it is unlikely to predict accurately long-term corrosion behavior under storage and disposal conditions by simply extrapolating the high temperature corrosion data. (authors)
Grid-to-rod fretting wear study of SiC/SiC composite accident-tolerant fuel claddings using an autoclave fretting bench test
Grid-to-rod-fretting (GTRF) in pressurized water reactors (PWRs) is known to cause wear and surface damage on the fuel claddings, potentially leading to radioactive leakage. One of the accident-tolerant fuel (ATF) concepts is to use advanced cladding materials that could withstand higher temperatures. Here, we investigated the wear behavior of candidate silicon carbide (SiC)-based composite claddings with different levels of surface finish in fretting against a commercial ZIRLO alloy grid using a unique bench-scale autoclave GTRF rig. The experiments mimicked the environment in an industrial full-assembly PWR simulator. Fretting tests were conducted with a realistic load (~0.5 N) in deionized water under a pressure of 20–23 bar at 204 °C for 100 h. While the SiC/SiC composite claddings showed significantly higher wear resistance than the commercial ZIRLO alloy cladding as expected, the smoother versions experienced surprisingly higher wear than the much softer counterface, ZIRLO grid. The wear mechanism of the SiC/SiC cladding was attributed to the SiC wear debris that was trapped at the fretting interface causing both 3-body and 2-body (embedded into the grid surface) abrasion of the cladding. Rougher SiC/SiC claddings had less material loss but caused more wear on the ZIRLO grid. Finally, pre-oxidized ZIRLO grid showed better compatibility with the SiC/SiC cladding to protect both the cladding and grid as a result of reduced wear debris trapping.
Comparison of woven and stitched out-of-autoclave E-glass/epoxy composites subjected to quasi-static and cyclic tensile loads
Tensile quasi-static and fatigue behaviors of out-of-autoclave, quasi-isotropic, E-glass/epoxy composites with woven and stitched fiber architectures are compared. Some specimens were cyclically loaded to failure, while others were tested for residual modulus and ultimate strength. Both laminates survived 10 7 cycles at a maximum stress of 94.8 MPa but failed prior to 10 7 cycles at a maximum stress greater than or equal to 124.1 MPa. For the stress-lifetime diagram and residual strength, the woven laminate had superior properties below 10 4 cycles and the stitched laminate had superior properties above 10 5 cycles. While intralaminar crack density was higher in the stitched laminate, the woven laminate demonstrated a higher percentage of delaminated area.
The Development of High Temperature Thermoplastic Composite Materials for Additive Manufactured Autoclave Tooling
In this work, ORNL and Techmer investigated and screened different high temperature thermoplastic reinforced materials to fabricate composite molds for autoclave processes using Additive Manufacturing (AM) techniques. This project directly led to the development and commercial release of two printable, high temperature composite materials available through Techmer PM. These new materials are targeted for high temperature tooling made via large scale additive manufacturing.
Demonstrate HTIR performance in flowing autoclave for fuel center line temperature measurement in PWR conditions [Slides]
The results from the ATF-2 fuel pin mockup test in the INL's flowing autoclave system (FAS) is presented. By instrumenting the fuel pins with high-temperature, irradiation-resistant thermocouples, the fuel center line can be measured directly. This test shows performance of the compression seals and leak tightness of the temperature probes.
A scalable and autoclavable oxygen nanosensor platform for metabolic monitoring of Saccharomyces cerevisiae in a bioreactor and other in situ systems
Polymer-encapsulated dye nanoparticle sensors are a valuable approach to achieving in situ analyte measurements with luminescence; however, typical emulsion-based nanosensors are poorly suited for large-scale biological samples due to limitations of synthesis scalability and stability. Branched polyethylenimine (PEI) is a versatile polymer scaffold ideal for constructing nanoparticles with various covalently conjugated moieties due to their high density of reactive primary amines, high water solubility, and biological stability. In this work, we used branched polyethylenimine as a scaffold-based approach for making a stable and scalable ratiometric oxygen sensor. Pt (II) tetracarboxyporphine was used as an oxygen-sensing dye and coumarin 343 as a reference dye, all covalently linked to the PEI scaffold producing a product that could withstand sterilization procedures and easily be scaled. To minimize toxicity from the PEI scaffold, we conjugated it with 2000 MW PEG. The applicability of the sensors was demonstrated in a 200 mL Saccharomyces cerevisiae yeast culture, using orthogonal luminescent and electrochemical oxygen measurements to validate sensor response and measure the metabolic activity of the yeast in our culture. Further, this approach was able to match the sensitivity of our electrochemical measurements while improving upon drawbacks of other luminescent methods of oxygen detection, demonstrating effective monitoring for at least 20 h. Our scaffold-based approach is a modular and easily translatable technology that could be useful in various biotechnological applications.